EP3748019A1 - Procédé résistant au recuit de relâchement de contraintes pour une fabrication d'acier au silicium orienté à faible perte de fer - Google Patents

Procédé résistant au recuit de relâchement de contraintes pour une fabrication d'acier au silicium orienté à faible perte de fer Download PDF

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EP3748019A1
EP3748019A1 EP18904474.6A EP18904474A EP3748019A1 EP 3748019 A1 EP3748019 A1 EP 3748019A1 EP 18904474 A EP18904474 A EP 18904474A EP 3748019 A1 EP3748019 A1 EP 3748019A1
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Prior art keywords
silicon steel
annealing
steel sheet
laser
grain
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EP3748019A4 (fr
EP3748019B1 (fr
Inventor
Shuangjie Chu
Guobao Li
Yongjie Yang
Zipeng Zhao
Changsong MA
Kanyi Shen
Meihong Wu
Yaming Ji
Huabing ZHANG
Zhuochao Hu
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Baoshan Iron and Steel Co Ltd
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Baoshan Iron and Steel Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0206—Manufacturing of magnetic cores by mechanical means
    • H01F41/0233—Manufacturing of magnetic circuits made from sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/02—Positioning or observing the workpiece, e.g. with respect to the point of impact; Aligning, aiming or focusing the laser beam
    • B23K26/06—Shaping the laser beam, e.g. by masks or multi-focusing
    • B23K26/0604—Shaping the laser beam, e.g. by masks or multi-focusing by a combination of beams
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/02—Positioning or observing the workpiece, e.g. with respect to the point of impact; Aligning, aiming or focusing the laser beam
    • B23K26/06—Shaping the laser beam, e.g. by masks or multi-focusing
    • B23K26/062—Shaping the laser beam, e.g. by masks or multi-focusing by direct control of the laser beam
    • B23K26/0622—Shaping the laser beam, e.g. by masks or multi-focusing by direct control of the laser beam by shaping pulses
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/08—Devices involving relative movement between laser beam and workpiece
    • B23K26/082—Scanning systems, i.e. devices involving movement of the laser beam relative to the laser head
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/36—Removing material
    • B23K26/362—Laser etching
    • B23K26/364—Laser etching for making a groove or trench, e.g. for scribing a break initiation groove
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/06—Surface hardening
    • C21D1/09—Surface hardening by direct application of electrical or wave energy; by particle radiation
    • C—CHEMISTRY; METALLURGY
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    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/26—Methods of annealing
    • C21D1/30—Stress-relieving
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D10/00—Modifying the physical properties by methods other than heat treatment or deformation
    • C21D10/005—Modifying the physical properties by methods other than heat treatment or deformation by laser shock processing
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1216—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the working step(s) being of interest
    • C21D8/1222—Hot rolling
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1216—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the working step(s) being of interest
    • C21D8/1233—Cold rolling
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
    • C21D8/1255—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest with diffusion of elements, e.g. decarburising, nitriding
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
    • C21D8/1272—Final recrystallisation annealing
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1277—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1277—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
    • C21D8/1283—Application of a separating or insulating coating
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/16—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of sheets
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets

Definitions

  • the present invention relates to a method for manufacturing stress-relief-annealing-resistant, low-iron-loss grain-oriented silicon steel, and more particularly to a method for manufacturing stress-relief-annealing-resistant, laser-scoring grain-oriented silicon steel.
  • the orientation degree of grains of grain-oriented silicon steel has been raised to a relatively high level by metallurgical methods, and the average deviation angle of grain orientation in Hi-B steel is less than 5°. Therefore, the technique to improve the performance of grain-oriented silicon steel mainly focuses on the improvement of coating tension and scoring process.
  • Scoring on the surface of grain-oriented silicon steel can refine magnetic domains, thereby reducing iron loss.
  • the scoring technique can be divided into two categories.
  • One type is the scoring technique that is not resistant to stress-relief annealing, also known as non-heat-resistant scoring technique.
  • a linear thermal stress region is formed on the surface of the silicon steel sheet at a certain spacing by a laser, a plasma beam, an electron beam, or the like to cause sub-magnetic domains around the region, thereby reducing the width of the main magnetic domains and achieving the purpose of reducing iron loss.
  • the refinement of magnetic domains by this technique disappears after stress-relief annealing.
  • the products thus obtained are usually used to manufacture laminated iron core transformers that do not require annealing.
  • the other type is the scoring technique that is resistant to stress-relief annealing, also known as heat-resistant scoring technique.
  • the existing industrial technique mainly involves the formation of linear strain zones, i.e., linear grooves, on the surface of the grain-oriented silicon steel substrate by mechanical or electrochemical erosion, etc., to redistribute the magnetostatic energy of the system around the strain zone and reduce the width of the main magnetic domains. Thus, the reduction of iron loss is achieved.
  • the refinement of magnetic domains does not deteriorate after stress-relief annealing, and the product thus obtained can be used to manufacture wound core transformers that require stress-relief annealing.
  • heat-resistant scoring grain-oriented silicon steel products were usually produced by mechanical methods.
  • linear grooves are formed on the surface of the grain-oriented silicon steel by mechanical scoring such as gear rollers, so as to achieve heat-resistant scoring.
  • the grain-oriented silicon steel substrate with a silicon content of about 3% and the magnesium silicate layer on the surface have extremely high hardness, and the gear rollers are easy to wear, resulting in uneven iron loss of the entire roll, and the production cost is extremely high, which is not conducive to mass production.
  • electrolytic corrosion is used to form heat-resistant scoring grain-oriented silicon steel.
  • the grain-oriented silicon steel sheet with an underlayer is linearly processed by a laser or the like to expose the metal substrate in the region.
  • the grain-oriented silicon steel sheet is then immersed in the electrolyte to form an electrode pair between the silicon steel sheet and the electrode.
  • the substrate is electrolytically etched by alternately controlling the positive and negative changes in the electrode potential so that the region forms linear grooves.
  • the grooves are filled with metal(s) such as Al that has a different thermal expansion coefficient from the silicon steel sheet substrate by electrophoresis or spray.
  • metal(s) such as Al that has a different thermal expansion coefficient from the silicon steel sheet substrate by electrophoresis or spray.
  • the silicon steel sheet substrate is cured and sintered at 650 °C.
  • the difference between the thermal expansion coefficients of the filler and the substrate results in the formation of stress in this linear region, and P17/50 can be reduced by 8-12%.
  • the procedures and process control of the above two methods are extremely complicated, the manufacturing cost is high, and the processing speed is limited.
  • the above laser heat-resistant scoring methods all use traditional continuous or pulsed lasers. Due to the high melting point and the fast heat conduction speed of steel, the methods of using traditional lasers to achieve heat-resistant scoring all result in different degrees of melt accumulation, and there may even be thermally deformation of the steel sheet and extremely low laser energy utilization efficiency. Moreover, the quality of the score is difficult to control, resulting in unstable magnetic properties of the product, and the improvement effect is greatly restricted.
  • the laser heat-resistant magnetic domain refinement techniques reported so far all use pulse laser light sources or continuous laser light sources.
  • the principle of such technique is to use a high-energy beam laser to heat the steel plate to be the melting temperature or more, and thus melt the substrate metal and form splashing of fine molten metal droplets, or the substrate metal is directly heated to vaporize, thereby forming grooves on the surface of the silicon steel sheet.
  • An object of the present invention is to provide a method for manufacturing stress-relief-annealing-resistant, low-iron-loss grain-oriented silicon steel.
  • the method overcomes the shortcomings of the existing laser heat-resistant scoring process, and greatly reduces the thermal influence, melt protrusion, and heat-affected zone during the laser scoring process, and there is no plate shape deterioration.
  • the produced grain-oriented silicon steel sheet has a remarkable magnetic domain refinement effect, low iron loss and no reduction in lamination coefficients.
  • a method for manufacturing stress-relief annealing resistant, low-iron-loss grain-oriented silicon steel comprising: subjecting a silicon steel to iron smelting, steel smelting, continuous casting, hot rolling, single or double cold rolling, followed by decarburization annealing, coating a MgO-based separation agent on the surface of the steel, high-temperature annealing, finally, applying an insulating coating on the surface of the steel and performing hot stretching, temper rolling and annealing, thereby obtaining a finished product, wherein the method further comprising: carrying out, by means of a pulse laser, scanning grooving on a single surface or both surfaces of the resultant silicon steel sheet after cold rolling, or after decarburizing annealing, or after high temperature annealing or after hot stretching, temper rolling and annealing, and forming several grooves parallel with each other in a rolling direction of the silicon steel sheet; wherein a single pulse time width of the pulse laser is 100 ns or less, and the peak energy
  • scanning grooving is performed on a single surface or both surfaces of the silicon steel sheet after hot stretching, temper rolling and annealing; after the grooving, silicon steel sheet is coated with secondary insulating coating(s) on one or both surfaces thereof and is then sintered.
  • the grooves formed on the surface of the silicon steel sheet of the present invention have a depth of 5 to 35 ⁇ m and a width of 8 to 310 ⁇ m.
  • the height of the deposits formed by laser processing on both sides of the grooves is 2.5 ⁇ m or less, and the angle between the grooves and the lateral direction of the silicon steel sheet is 45° or less.
  • the spacing between adjacent grooves in the rolling direction of the silicon steel sheet is 1 to 10 mm.
  • the spacing between adjacent grooves in the rolling direction of the silicon steel sheet is 2 to 20 mm.
  • the wavelength of the laser light wave is 0.3 ⁇ 3 ⁇ m.
  • Conventional grain-oriented silicon steel is formed into finished products through the following steps and then subcontracted for delivery: iron smelting, steel smelting, continuous casting, hot rolling, single or double cold rolling to the final thickness, and followed by decarburization annealing, coating a MgO-based separation agent on the surface, and high-temperature annealing to form a complete secondary recrystallization and magnesium silicate underlayer, and finally, coating an insulating coating on its surface and performing hot stretching, temper rolling and annealing.
  • the invention is suitable for the manufacture of conventional grain-oriented silicon steel.
  • the method of the invention utilizes instantaneous high-energy pulse laser to scan and form grooves on the surface of the silicon steel sheet.
  • the groove processing can be performed before or after decarburization annealing, or before or after hot stretching, temper rolling and annealing.
  • Grain-oriented silicon steel sheets or strips that are scored after hot stretching, temper rolling and annealing may or may not be coated secondary insulating coating(s) and sintered after being grooved.
  • the inventors have found through research that, using a pulse laser with a small time width can increase the instantaneous energy, and effectively control the deformation of the steel plate caused by thermal melting and diffusion. Moreover, the shortening of the pulse time width can significantly reduce the thermal effect, thermal melting and metal splashing of the material.
  • the time width of a single laser pulse is 100 ns or less
  • the instantaneous pulse energy in the laser is greatly increased
  • the depth of the groove obtained by processing can be in the range of 5 ⁇ 35 ⁇ m
  • the height of the deposits on both sides can be 2.5 ⁇ m or less, thereby obtaining grain-oriented silicon steel products with excellent magnetic properties and good lamination coefficients.
  • the wavelength of the pulse laser used is not limited, but preferably ranges from 0.3 to 3 ⁇ m. Within this preferred range, the laser absorption coefficient of the grain-oriented silicon steel material is relatively high, so that better processing efficiency can be obtained.
  • the peak energy density of a single pulse of the pulse laser used in the present invention is 0.05 J/cm 2 or more. This is because when the single pulse peak energy density of the pulse laser is less than 0.05 J/cm 2 , the laser energy is too low, which results in extremely low grooving efficiency on the surface of grain-oriented silicon steel, and even may not form grooves, and it has no application value.
  • the laser beam spot used for processing may be a single beam spot or a combination of a plurality of beam spots.
  • the shape of the beam spot(s) is/are circular or elliptic;
  • the diameter a of the circular beam spot and the diameter a of the elliptical beam spot in the laser scanning direction are in the range of 5 ⁇ m ⁇ 1 mm, and the diameter b of the elliptical beam spot in a direction perpendicular to the laser scanning direction is 5 ⁇ m ⁇ 300 ⁇ m;
  • the combination of a plurality of beams spots is composed of a plurality of beam spots linearly arranged along the scanning direction, with the number of beam spots being 2 to 300;
  • the average value of the spacing d m between the beam spots in the scanning direction in the combination of a plurality of beams spots formed on the surface of the steel plate is between c / 5 and 5c, where c is the average diameter of the
  • the spacing is limited to this range, so that the spacing of the laser beams brings cooling time to prevent the accumulation of melt on the surface of the material due to the excessively high temperature.
  • the mode of the single beam spot or the combination of a plurality of beams spots reduces the scan times of the laser and improves the laser scanning efficiency.
  • the inventors have found through research that, in order to prevent the formation of melt deposits on both sides of the groove, it is necessary to appropriately reduce the energy density of the single beam spot and achieve the desired depth of the groove through multiple scannings.
  • the inventor determined the number of laser beam spots and the scan times through experiments, that is, when the scanning grooving is carried out at the same position on the steel sheet, the product of the number of laser beam spots and the scan times is 5 or more, which achieves the dual purpose of controlling the accumulation of melt and reducing the iron loss.
  • the product is less than 5
  • the purpose of reducing the iron loss can be achieved by increasing the laser energy, but the thermal melting phenomenon is serious.
  • the melt accumulates on both sides of the grooves, greatly reducing the lamination coefficient of the silicon steel sheet. If the thermal melting is controlled by reducing the energy, the desired groove depth cannot be achieved, nor can the purpose of significantly refining the magnetic domains and reducing the iron loss of the silicon steel sheet be achieved.
  • the energy flux density of a single laser beam in a single scan E s is 1 J/cm 2 to 100 J/cm 2 .
  • an instantaneous high-energy pulse laser is used to perform linear micromachining on a single surface or both surfaces of a silicon steel sheet to form grooves.
  • the groove has a depth of 5 ⁇ 30 ⁇ m, and a width of 8-310 ⁇ m.
  • the depth of the groove is less than 5 ⁇ m or the width of the groove is less than 8 ⁇ m, the effect of scoring on the refinement of magnetic domains is not obvious, and the reduction of iron loss is limited.
  • the depth of the groove is more than 30 ⁇ m or the width is more than 310 ⁇ m, the magnetic flux leakage at the grooves is large, resulting in a decrease in magnetic induction, and multiple scans are needed for forming the desired groove size, that is, the laser scoring efficiency is low.
  • the spacing between adjacent grooves in the rolling direction when a single surface of the grain-oriented silicon steel sheet is grooved, the spacing between adjacent grooves in the rolling direction is 1 to 10 mm. When both surfaces of the grain-oriented silicon steel sheet are grooved, the spacing between adjacent grooves in the rolling direction is 2 to 20 mm.
  • the spacing between adjacent grooves in the rolling direction when the spacing between adjacent grooves in the rolling direction is less than 1 mm, the number of score lines is large, which significantly reduces the magnetic induction of the grain-oriented silicon steel sheet.
  • the spacing between adjacent grooves in the rolling direction is more than 10 mm, the refinement of the magnetic domain by the score lines is limited, and the reduction of iron loss is not obvious.
  • the spacing between adjacent grooves in the rolling direction when the spacing between adjacent grooves in the rolling direction is less than 2 mm or more than 20 mm, the above issues will also occur.
  • an instantaneous high-energy pulse laser source is used to perform non-hot-melt processing to form grooves, obtains heat-resistant scoring grain-oriented silicon steel with low iron loss, and greatly reduces the heat influence, the melt protrusion and the heat-affected zone during the groove processing.
  • the edges of the scored grooves are flat, the height of the protrusions or deposits is small, and the plate shape is good.
  • the magnetic domain refinement effect of the manufactured grain-oriented silicon steel sheet is remarkable, the iron loss is low and the lamination coefficient is maintained. Therefore, wound core transformers made of the grain-oriented silicon steel sheet have the characteristics of low loss and low noise.
  • an instantaneous high-energy pulse laser is used to score the grain-oriented silicon steel sheet, and the product of the number of laser beam spots and the scan times thereof is much more than that of existing laser scoring methods.
  • the method of the invention not only greatly reduces the thermal effect and heat accumulation, ensures that the steel plate is not deformed, but also effectively controls the deposits and metal splashes on both sides of the groove.
  • the height of deposits on both sides of the groove are controlled to 2.5 ⁇ m or less, ensuring that the lamination coefficient of grain-oriented silicon steel does not decrease, and thus obtain better score quality and finished product performance with better laser energy efficiency.
  • the produced grain-oriented silicon steel sheet has a remarkable magnetic domain refinement effect, low iron loss and no reduction in lamination coefficient.
  • FIG. 1 is a schematic diagram of the single laser beam spot and the combination of a plurality of beams spots used in the present invention.
  • the grain-oriented silicon steel was subjected to iron smelting, steel smelting and continuous casting to obtain a billet containing C: 0.07%, Si: 3.1%, Mn: 0.14%, Al: 0.020%, N: 0.01%, S: 0.01% in mass%. Then, the billet was subjected to hot rolling and single cold rolling to achieve a final thickness of 0.23 mm. After performing decarburization annealing to form a surface oxide layer, coating an annealing separation agent containing MgO as the main component on the surface, and high-temperature annealing at 1250 °C for 20 hours. After washing away the unreacted residual MgO, laser heat-resistant scoring was performed on a single surface of the steel plate.
  • the parameters of laser scanning scoring were as follows: the laser pulse time width was 10 ns, the laser wavelength was 1066 nm, the repetition frequency was 800 KHz, the diameter b of the beam spot perpendicular to the scanning direction was 50 ⁇ m, the spacing d m between beam spots in a group of beam spots was 10 ⁇ m, and the number of beam spots was 5.
  • the depth of the grooves formed by scoring was controlled to be 15-18 ⁇ m, and the width was controlled to be 50-55 ⁇ m.
  • the angle between the groove and the lateral direction of the steel plate is 8°, and the spacing between adjacent grooves in the rolling direction is 4.5 mm. Table 1 shows the parameters of specific scoring process. After the scoring was completed, final annealing was performed to apply the tension coating.
  • Epstein 0.5 kg method in GB/T3655-2008 was used for magnetic measurement of the silicon steel sheets.
  • GB/T19289-2003 was used to determine the lamination coefficient of the silicon steel sheets.
  • the measurement results of Examples 1-10 and Comparative Examples 1-3 are shown in Table 2.
  • the iron loss P17/50 of the silicon steel sheet after scoring is 0.75 W/kg or less, and the lamination coefficient remains 95% or more.
  • the energy flux density of a single laser beam in a single scan is outside the range of the present invention.
  • the iron loss P17/50 is good in Comparative Examples 1 and 2, the lamination coefficient decreases significantly.
  • the peak energy density of a single pulse is too low, which results in poor scoring effects (when the scan times reaches 30, the depth of the grooves formed by laser scoring is only 3.3 ⁇ m) and high iron loss, and thus it has no industrial value.
  • the grain-oriented silicon steel was subjected to iron smelting, steel smelting and continuous casting to obtain a billet containing C: 0.05%, Si: 3.7%, Mn: 0.10%, Al: 0.03%, N: 0.016%, S: 0.013% in mass%. Then, the billet was subjected to hot rolling and single cold rolling to achieve a final thickness of 0.26 mm. After performing decarburization annealing to form a surface oxide layer, coating an annealing separation agent containing MgO as the main component on the surface, and performing high-temperature annealing at 1250 °C for 20 hours. After washing away the unreacted residual MgO, hot stretching, temper rolling and annealing was performed to apply a tension coating.
  • the laser scoring was performed on both the upper and lower surfaces of the steel plate.
  • the laser wavelength is 533 nm and the repetition frequency is 600 KHz.
  • the pulse width, laser output power, beam spot size, beam spot combination, scanning speed, scan times and other parameters were adjusted to achieve the desired scoring effect.
  • Table 3 shows the parameters of specific scoring process.
  • the grooves are perpendicular to the rolling direction of the steel plate.
  • the spacing between adjacent grooves in the rolling direction is 6 mm.
  • the insulating coating was applied again and dried and sintered to form the final grain-oriented silicon steel sheet.
  • Epstein 0.5 kg method in GB/T3655-2008 was used for magnetic measurement of the silicon steel sheets.
  • GB/T19289-2003 was used to determine the lamination coefficient of the silicon steel sheets.
  • the measurement results of Examples 11-20 and Comparative Examples 4-12 are shown in Table 4.
  • the height of the protrusions on both sides of the groove formed by scoring is 2.5 ⁇ m or less, and the magnetic properties of the silicon steel sheet are good after stress-relief annealing.
  • the height of the protrusions on both sides of the groove formed by the scoring is more than 2.5 ⁇ m, the magnetic induction or the lamination coefficient is significantly reduced.
  • the grain-oriented silicon steel was subjected to iron smelting, steel smelting and continuous casting to obtain a billet containing C: 0.09%, Si: 2.9%, Mn: 0.12%, Al: 0.019%, N: 0.016%, S: 0.012% in mass%. Then, the billet was subjected to hot rolling and single cold rolling to achieve a final thickness of 0.22 mm. After performing decarburization annealing to form a surface oxide layer, linear microgrooves were scored on the surface of the steel plate using a pulse laser with a pulse time width of 0.5 nanoseconds. The output power of the laser was 100 W, the wavelength of the light wave was 533 nm, and the repetition frequency was 200 KHz.
  • the beam spot focused on the surface of the steel plate was circular.
  • the laser was a combination of multiple beam spots, and the number of beam spots was 20.
  • the spacing between beam spots in the group of beam spots was 40 ⁇ m, and the laser scanning speed was 10 m/s.
  • the scan times, scanning direction, and offset direction of scanning were adjusted to obtain different groove depth, width, and the angle between the score line and the lateral direction of the steel plate. Table 5 shows the parameters of specific scoring process.
  • the above samples were subjected to a decarburization annealing process at a temperature of 830°C to form a surface oxide layer. Then, MgO separation agent was applied to the surface of the steel plate. After the steel plate was made into steel coils, it was kept under high temperature annealing conditions at 1200°C for 20 hours. Finally, after washing away the residual MgO, an insulating coating was applied on the surface of the steel coil, and the final hot stretching, temper rolling and annealing was performed to obtain a finished silicon steel sheet.
  • Epstein 0.5 kg method in GB/T3655-2008 was used for magnetic measurement of the silicon steel sheets.
  • GB/T19289-2003 was used to determine the lamination coefficient of the silicon steel sheets.
  • the measurement results of Examples 21-30 and Comparative Examples 13-21 are shown in Table 6.
  • the present invention uses instantaneous high-energy laser to score the silicon steel surface.
  • the method of the invention has the advantages of high processing efficiency and good scoring effect, and is particularly suitable for the manufacture of high-efficiency coiled iron core transformers, which can effectively save the power loss caused by transmission and distribution in the power grid and has good applicability. Table 1.
  • Example 1 Magnetic properties of silicon steel sheets after stress-relief annealing P17/50 (W/kg) B8 (T) Lamination coefficient (%)
  • Example 1 0.735 1.912 97.3
  • Example 2 0.748 1.909 97.5
  • Example 3 0.736 1.907 96.5
  • Example 4 0.742 1.91 96.2
  • Example 5 0.729 1.908 95.9
  • Example 6 0.75 1.914 96.8
  • Example 7 0.741 1.909 97.6
  • Example 8 0.733 1.909 97.2
  • Example 9 0.746 1.911 96.9
  • Example 10 0.748 1.908 95.4 Comparative Example 1 0.763 1.901 93.8 Comparative Example 2 0.742 1.905 94.2 Comparative Example 3 0.886 1.92 97.5 Table 3.

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4064372A4 (fr) * 2019-11-18 2023-12-20 Sumitomo Metal Mining Co., Ltd. Élément magnétostrictif et procédé de production d'élément magnétostrictif

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2764777C1 (ru) * 2021-01-26 2022-01-21 Федеральное государственное бюджетное учреждение науки Институт электрофизики и электроэнергетики Российской академии наук (ИЭЭ РАН) Способ обработки поверхности цветного металла путем формирования микрорельефа
CN113564321B (zh) * 2021-07-09 2024-04-12 首钢智新迁安电磁材料有限公司 一种取向硅钢的磁畴细化方法及应用
JP7053933B1 (ja) 2021-08-31 2022-04-12 Dmg森精機株式会社 ワーク加工方法およびレーザ加工機
CN113960085A (zh) * 2021-09-22 2022-01-21 中国工程物理研究院激光聚变研究中心 一种有色金属多晶材料晶粒尺寸的高效测量方法
CN113957222B (zh) * 2021-10-26 2023-06-30 无锡普天铁心股份有限公司 一种降低取向硅钢铁损的方法
CN117415448A (zh) * 2022-07-11 2024-01-19 宝山钢铁股份有限公司 一种用于低铁损取向硅钢板的激光刻痕方法及取向硅钢板
CN115519226B (zh) * 2022-11-28 2023-02-28 中国航空制造技术研究院 一种提高电子束熔丝成形制件精度的成形装置及方法
CN115767937B (zh) * 2022-12-07 2023-07-21 广东工业大学 一种基于减成法原理的精细线路修复方法

Family Cites Families (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4535218A (en) * 1982-10-20 1985-08-13 Westinghouse Electric Corp. Laser scribing apparatus and process for using
JPS60103183A (ja) 1983-11-09 1985-06-07 Kawasaki Steel Corp 歪取り焼鈍によつて特性が劣化しない低鉄損の方向性けい素鋼板およびその製造方法
JPS61117218A (ja) 1984-11-10 1986-06-04 Nippon Steel Corp 低鉄損一方向性電磁鋼板の製造方法
GB2208871B (en) * 1987-08-22 1991-03-27 British Steel Plc Processing grain-oriented "electrical" steel
IN171547B (fr) 1988-03-25 1992-11-14 Armco Advanced Materials
US5146063A (en) 1988-10-26 1992-09-08 Kawasaki Steel Corporation Low iron loss grain oriented silicon steel sheets and method of producing the same
JP2563729B2 (ja) 1992-08-07 1996-12-18 新日本製鐵株式会社 パルスｃｏ２レーザを用いた方向性電磁鋼板の鉄損改善方法および装置
US5296051A (en) 1993-02-11 1994-03-22 Kawasaki Steel Corporation Method of producing low iron loss grain-oriented silicon steel sheet having low-noise and superior shape characteristics
EP0870843A1 (fr) * 1995-12-27 1998-10-14 Nippon Steel Corporation Tole d'acier magnetique ayant d'excellentes proprietes magnetiques, et son procede de fabrication
EP1342818B1 (fr) 2002-03-04 2016-09-07 Nippon Steel & Sumitomo Metal Corporation Procédé et dispositif pour le décapage électrolytique continu de bandes métalliques du type à électrification indirecte
JP4398666B2 (ja) 2002-05-31 2010-01-13 新日本製鐵株式会社 磁気特性の優れた一方向性電磁鋼板およびその製造方法
WO2011007771A1 (fr) * 2009-07-13 2011-01-20 新日本製鐵株式会社 Procédé de fabrication d'une plaque d'acier électromagnétique à grains orientés
CN102834529A (zh) 2010-04-01 2012-12-19 新日本制铁株式会社 方向性电磁钢板及其制造方法
BR112013002087B1 (pt) * 2010-07-28 2021-03-23 Nippon Steel Corporation Chapa de aço elétrico com grão orientado e método de produção da mesma
CN104099458B (zh) 2010-09-09 2016-05-11 新日铁住金株式会社 方向性电磁钢板的制造方法
CN102477484B (zh) 2010-11-26 2013-09-25 宝山钢铁股份有限公司 一种快速激光刻痕方法
CA2860667C (fr) * 2012-01-12 2020-04-28 Nucor Corporation Traitement d'acier electrique sans recuit intermediaire apres le laminage a froid
US9761360B2 (en) * 2012-03-29 2017-09-12 Jfe Steel Corporation Method of manufacturing grain oriented electrical steel sheet
EP3205738B1 (fr) * 2014-10-06 2019-02-27 JFE Steel Corporation Tôle d'acier électromagnétique à grains orientés et à faible perte dans le noyau et son procédé de fabrication
CN106282512B (zh) * 2015-05-11 2018-03-30 宝山钢铁股份有限公司 低噪音变压器用取向硅钢片制造方法
KR101659350B1 (ko) 2016-02-11 2016-09-23 주식회사 포스코 방향성 전기강판 및 그 제조방법
CN105925884B (zh) * 2016-05-30 2018-03-09 宝山钢铁股份有限公司 一种高磁感、低铁损无取向硅钢片及其制造方法
CN107502723A (zh) * 2017-09-15 2017-12-22 武汉钢铁有限公司 通过激光双面刻痕降低取向硅钢铁损的方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4064372A4 (fr) * 2019-11-18 2023-12-20 Sumitomo Metal Mining Co., Ltd. Élément magnétostrictif et procédé de production d'élément magnétostrictif

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